Apeabatus fob oenebating etheb



Jun e 1 1926.

F. E. LICHTENTHAELER APPARATUS FOR GENERATING ETHER June 1,1926. 1,587,161

F. E. LICHTENTHAELER V APPARATUS FOR GENERATING mun Filed Sept. 2a. 1923 2 Sheets-Sheet 2 Patented June 1, 1926.

OFFIE.

APPARATUS FOR GENERATING ETHEB.

Application filed September 28, 1.928. Serial No. 885,408.

The present invention relates to apparatus for generating ether and more particularly to apparatus for the continuous generation of ether by the interaction of sulphuric acid and alcohol.

The commercial manufacture of ethyl 1 ether is ordinarily carried out by the well known reactions between ethyl alcohol and sulphuric acid. Although the reactions may be considered as taking place in two steps, namely, the formation of ethyl sulphuric acid by contact ofsulphuric acid and alcohol, and the decomposition of the ethyl sulphuric acid by heat, these steps take place practically simultaneously, resulting in the evolution of ether and the generation of the sulphuric acid in its original form.

The standard ether generator in which the ether forming reactions are carried out consists merely of a lead or lead lined receptacle within which a charge of sulphuric acid and alcohol is placed. The mixture is heated to approximately 130 C. by means of an internal steam coil which because of its external contact with the sulphuric acid is ordinarily constructed of lead. The alcohol is fed into the receptacle in a continuous stream and the evolved ether vapor is continuously withdrawn, being subsequently passed through neutralizing and rectifying apparatus of any usual or preferred form. This type of ether generator although exceedingly simple in construction and. operation possesses many important disadvantages, among the principal of which are the weakness and liability to rupture of the lead heating coils. Lead pipe is known to be extremely weak under internal pressure .and even when made of considerable thickness is liable to splitting or other breakage. Furthermore the construction of the generator does not lend itself to the ready replacement of heating coils. Accordingly the breakage or corrosion of a heating coil entails serious delays with consequent high expense. In addition to the inconveniences due to failure of the heating coils, the apparatus is also open to the disadvantage that it is inefficient even under most favorable operating conditions. This is due to the non-uniform distribution of heat throughout the alcohol and acid mixture and consequent localized overheating and sluggish circulation. It has been found that the maximum temperature occurs at the steam inlet and decreases progressively through the heating coil, thus causing side reactions and undesirable foaming at the overheated points, and failing to give the propercirculation and intimate contact between the reacting substances throughout the remainder of the mass, so that the yields are reduced by the passage of considerable unconverted alcohol over with the ether.

The object of the present invention is to reorganize and improve the construction of apparatus for generating ether with a View of obtaining maximum yields and of provlding a. generator in which replacements and repairs may be made during the normal operation of the apparatus and with a mimmum of inconvenience and expense. To this end, the invention consists in the apparatus for generating ether hereinafter described and particularly defined in the claims. ,1

In the accompanying drawings illustratmg the preferred form of the invention, Fig. 1 is a side elevation of the improved ether generator; Fi 2 is a front elevation of the generator; ig. 3 is a detail view showing the construction of the heating units; and Fig. 4 is a detail to be referred to.

The illustrated embodiment of the invention comprises a sulphuric acid reservoir 6 mounted'upon an elevated frame 8 and connected at the bottom to a downwardly inclined pipe 10 which is mounted on suitable standards 12 throughout its length. The reservoir 6 and pipe 10, being adapted for contact with sul huric acid, are constructed either wholly 0 leador with lead linings. The pipe 10 at its outer end connects with branch pipes 14 and 16 provided respectively with acid resisting valves 18 and 20. The pipes 14 and 16 connect respectively with headers 22 and 24 to which are connected the inclined heating units indicated generally at 26 and 28. As shown, the left hand heating unit comprises a. battery of three reaction conduits 30 presently to be described in detail, within which the entire ether evolving reaction takes place. The reaction conduits connect at their lower ends with the header 22 throu h pipes 32 and at their upper-ends with a eader 34 through I pipes 36. The right hand heating unit is of exactly similar construction consisting of reaction conduits having suitable connections with the lower header 24 and an upper header 38. The headers 34 and 38 connect through valves 40 and 42 with pipes 44 and 46, respectively, to a connection 48 leading directly into theupper portion of the reservoir. According to this construction, the sulphuric acid in the tank is caused to circulate from the bottom of the reservoir through the pipe 10 and then upwardly through the heating units in parallel into the upper part of the reservoir.

Each reaction conduit 30 comprises a generator tube 50 surrounded by a steam jacket 52 as shown in 3, the generator tube being coupled at its ends to the pipes 82 and 36. As illustrated in Fig. 4, the coupling is made by forming flanges 54 and 56 on the tubes 36 and 50 respectively, an asbestos gasket 58 being included between the flanges.- The steam jacket 52 is spaced from the generator tube by a collar 60. A flange ring 62 and flange 64 of the usual form serve to hold the coupling rigid, the latter flange being threaded on the steam jacket and the flange and flange ring being bolted together in the usual manner. The lower end of the generator tube is coupled to the pipe 32 in an exactly similar manner. Steam 1s introduced into the steam jackets of the heating units through suitable inlets, one being indicated at 66 for the left hand unit, and having the usual valves 68 and gage 70. The steam after circulating through the jackets is exhausted therefrom through an outlet 72 at the lower ends of the jackets. Alcohol is introduced into each generator tube for interaction with the sulphuric acid through a sparger pipe 74 extending upwardly into the generator tube and perforated at its upper end portion. The sparger pipe is separated from the pipe 32 and the generator pipe by suitable spacer blocks 76. Each sparger pipe is provided with a flange 78 at its lower end which permits a connection with a pipe 80 connecting with an alcohol .filling tube 82 at its upper end, the pipe 80 being supported along the side of its corresponding reaction conduit by clips 84. The parts thus far described which come in contact with sulphuric acid are necessarily of lead or other acid resisting material. The enerator tube 50 and sparger pipe 74 are of ead, but the steam jackets 52 not contacting with the acid are of iron which is better heat sensitive elements 92 in the upper headers for nieasurin the temperature of the sulphuric acid. lso, valves 94 of acid resisting material are provided at suitable points for permitting drainage of the apparatus.

The complete reaction by which ether is evolved and sulphuric acid generated takes place entirely within the generator tubes 50. The sulphuric acid is continuously circut lated through the tubes by thermosiphonic acti'on due to the heating of the conduits, and the proper amount of alcohol required for the reaction is introduced through the sparger pipes. The perforations in the sparger pipes permit thorough mixture of the alcohol and sulphuric acid, thereby forming intimate contact between the two liquids. The mixture of the liquids is thoroughly and uniformly heated by the application of steam outside of each generator tube separately. Furthermore, there is no danger of rupturing the lead pipes even under excessive steam pressures because lead is well able to resist the action of high compression forces. Owing to the flow of the liquids through the heating units in parallel, either one of the heating units may be isolated from the remainder of the system, thereby permitting repairs or replacements without seriously impairing the operation of the system. For example, the left hand heating unit 26 may be shut down by closing the valves 18 and 40 so that the entire flow passes through the right hand heating unit 28. Similarly the right hand unit may be shut down by closing the valves 20 and 42.

The invention, in its broader aspects, contemplates externally heated gener'ator tubes within which the entire ether evolving action takes place. Although the invention has been herein illustrated and described as embodied in a plurality of heating units each consisting of a bundle of parallel generator tubes, it will be understood that the particular construction ma be modified without departing from the roader features of the invention. For example, the generator tube, generically considered, consists of a tube supported entirely Within a casing through which steam is circulated, the entire reaction taking place within the tube as herein described.

The invention having been described, what is claimed is 1. An apparatus for generating ether having, in combination, a reservoir for sulphuric acid, a generator tube of acid resisting material,'connections from the ends of the generator tube to the top and bottom of the reservoir, a perforated pipe extending longitudinally into the generator tube for admitting alcohol within the tube, and means for externally heating the tube to cause the acid to circulate by thermosiphonic action from the bottom to the top of the reservoir a perforated pipe extended longitudinally through the tube and to promote the cominto the tube for admitting alcohol, and a plete ether forming reactions therein. steam jacket surrounding the tube for heating 2. An apparatus for generating ether havthe latter to promote the reaction between 5 ing, in combination, a sulphuric acid reserthe alcohol and acid to form ether, the acid voir, an inclined tube having connections at being continuously circulated through the its upper end with the reservoir, connections reservoir and tube by thermosiphonic action. from the bottom of the reservoir to the tube, FRANK E. LIOI-ITENTHAELER. 

